
7-Methoxy-8-hydroxy-4-phenylcouMarin synthesis
- Product Name:7-Methoxy-8-hydroxy-4-phenylcouMarin
- CAS Number:24258-36-4
- Molecular formula:C16H12O4
- Molecular Weight:268.26
Yield:24258-36-4 362 mg
Reaction Conditions:
with caesium carbonate in N,N-dimethyl-formamide at 10; for 1 h;
Steps:
6 Preparation of 4-phenyl-7-methoxy-8-hydroxycoumarin (II-ac)
Weigh 4-phenyl-7,8-dihydroxycoumarin 500mg dissolved in 5mL N, N-dimethylformamide,2.1 g of cesium carbonate,After stirring for 10 min,465 μL of methyl iodide was added dropwise,10 reaction,TLC monitors the progress of the reaction,1h after the reaction was over,Quench the reaction with water,With dilute hydrochloric acid to adjust the pH of the system to 3 to 4,A solid precipitation,After half an hour to filter,Collect the filter cake,Is the crude product.The crude product was separated by silica gel column,Mobile phase V petroleum ether: V ethyl acetate: V methanol = 3: 1: 0.1,The organic solvent was distilled off under reduced pressure,Dried under vacuum to give 362 mg of white solid,
References:
CN106518826,2017,A Location in patent:Paragraph 0048; 0049; 0050